CN101345296A - Preparation method and system for septum of lithium ion battery - Google Patents
Preparation method and system for septum of lithium ion battery Download PDFInfo
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- CN101345296A CN101345296A CNA2008100420430A CN200810042043A CN101345296A CN 101345296 A CN101345296 A CN 101345296A CN A2008100420430 A CNA2008100420430 A CN A2008100420430A CN 200810042043 A CN200810042043 A CN 200810042043A CN 101345296 A CN101345296 A CN 101345296A
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- lithium ion
- ion battery
- mineral oil
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 32
- 238000001125 extrusion Methods 0.000 claims abstract description 14
- 239000002480 mineral oil Substances 0.000 claims description 47
- 235000010446 mineral oil Nutrition 0.000 claims description 47
- 239000000758 substrate Substances 0.000 claims description 36
- 238000000605 extraction Methods 0.000 claims description 31
- 239000003963 antioxidant agent Substances 0.000 claims description 26
- 230000003078 antioxidant effect Effects 0.000 claims description 26
- 239000004698 Polyethylene Substances 0.000 claims description 22
- -1 polyethylene Polymers 0.000 claims description 22
- 229920000573 polyethylene Polymers 0.000 claims description 22
- 239000003431 cross linking reagent Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- 230000004888 barrier function Effects 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 238000001467 acupuncture Methods 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 239000002530 phenolic antioxidant Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 2
- 230000002457 bidirectional effect Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 29
- 235000006708 antioxidants Nutrition 0.000 description 21
- 229920001903 high density polyethylene Polymers 0.000 description 10
- 239000004700 high-density polyethylene Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 5
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 5
- 238000007766 curtain coating Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 229920000636 poly(norbornene) polymer Polymers 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 241001124569 Lycaenidae Species 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000014987 copper Nutrition 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a lithium ion battery diaphragm preparation method and a system; the lithium ion battery diaphragm preparation system comprises a mixing device, an extrusion device, a cooling and forming device, a bidirectional tensioning device, an extracting device, a thermal processing device and a slicing and packaging device which are sequentially connected. The preparation method of the invention can prepare ultra-thin batteries of 12 microns and has the advantages of good stability and long service life.
Description
Technical field
The present invention relates to a kind of preparation method and system, relate in particular to a kind of lithium ion battery separator preparation method and system.
Background technology
The chargeable lithium ion secondary cell has the characteristic of high-energy-density, long circulation life, memory-less effect, have again safety, reliable and can fast charging and discharging etc. advantage, thereby become the focus of novel power supply technical research in recent years.Because lithium ion battery is the free of contamination secondary cell of environmental type, meet the big growth requirement in countries nowadays energy environment protection aspect, increase sharply in the use amount of all trades and professions.Secondary lithium battery is also being brought into use aspect some high power batteries such as electric motor car, electric bicycle except that being widely used in digital electronic goods such as the daily mobile phone of knowing, notebook computer and MP3 in recent years at present.From calendar year 2001, global lithium ion battery output is increasing progressively rapidly with annual 40% speed.
Barrier film is the important component part of lithium ion battery, and its performance has determined interfacial structure, internal resistance of battery etc., directly influences the characteristic such as capacity, cycle performance of battery.The barrier film of excellent performance has important effect to the combination property that improves battery.But preparation technology in the past can cause the inhomogeneous and membrane thickness unevenness of lithium ion battery separator pore-forming, thereby influences the quality of lithium ion battery.
China Patent No. is that the patent of invention of 200710071919.X has announced that a kind of double screw extruder continuous polyethylene dissolving prepares the method for lithium ion battery separator.The method step that this double screw extruder continuous polyethylene dissolving prepares lithium ion battery separator is as follows:
One, ultra-high molecular weight polyethylene, high density polyethylene (HDPE) and mineral oil are together added in the continous batching coppers, stir with 10～60 rev/mins speed, raw material is mixed, wherein the mass ratio of ultra-high molecular weight polyethylene and high density polyethylene (HDPE) is 1: 1～15, and the gross mass of ultra-high molecular weight polyethylene and high density polyethylene (HDPE) and the mass ratio of mineral oil are 1: 5～15;
Two, mixture is added double screw extruder continuously, under 40～240 ℃ of conditions, ultra-high molecular weight polyethylene and high density polyethylene (HDPE) continuous-dissolution in double screw extruder is extruded with 50～250 rev/mins speed by double screw extruder in mineral oil more continuously;
Three, mixture is 1: 5～15 to be input in the slot die continuously according to the mass ratio of the gross mass of ultra-high molecular weight polyethylene and high density polyethylene (HDPE) and mineral oil;
Four, mixture is extruded into the curtain coating chill roll by slot die, the curtain coating thing that becomes band under 10～100 ℃ of conditions;
Five, the mineral oil of the belt surfaces that obtains of extraction step four;
Six, under 80～120 ℃ of conditions, ribbon is sent into biaxial orientation stretching machine 6 continuously and be drawn into film;
Seven, the mineral oil of the film surface that obtains of extraction step six;
Eight, under 80～120 ℃ of conditions, carried out thermal finalization 2～10 minutes;
Nine, with film with the rolling of 3～20 meters/component velocity, obtain lithium ion battery separator.
Said method has solved the uneven problem of film pore-forming in the conventional art, but also exists following defective:
The first, the mixture in the step 4 has only passed through one group of curtain coating chill roll in the said method, and the lithium ion battery separator thickness low LCL that causes it to make is even.
The second, said method has used extraction process twice, has increased cost of manufacture.
Three, the thickness of the lithium ion battery separator that makes with said method is between 15～60 millimeters, and it is blocked up that the minimum thickness of its film also shows.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery separator preparation method, to solve the defective that the lithium ion battery separator thickness low LCL is even and cost is higher that prior art makes.
Another object of the present invention is to provide a kind of lithium ion battery separator preparation system, to solve the defective that the lithium ion battery separator thickness low LCL is even and cost is higher that prior art makes.
In order to achieve the above object, the invention provides a kind of lithium ion battery separator preparation method, may further comprise the steps:
One, the speed with 40～300rpm in ultra high molecular polyethylene, crosslinking agent, antioxidant and the mineral oil proportioning adding by a certain percentage mixer is fully stirred raw material, wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35;
Two, will drop into double screw extruder by the step 1 mixture after being mixed and extrude continuously, form substrate with 100～250 ℃ of heating;
Three, making the substrate extruded from double screw extruder with 2～20 meters/minute speed is that 5～40 ℃ cooling forming machine carries out cooling forming by temperature range;
Four, with 2～20 meters/minute speed substrate is carried out horizontal stroke, vertical two-way simultaneous stretching by biaxial tension equipment, make substrate be drawn into film, the film thickness of drawing and forming reaches 30～100 μ m, and barrier film acupuncture intensity is 300～600gf;
Five, be that 1500～2500 millimeters film extracts mineral oil in the film by extraction tank with width;
Six, under 100～160 ℃ temperature, film carried out 1～3 minute heat treatment;
Seven, curling lithium battery diaphragm is cut packing.
According to the described lithium ion battery separator preparation method of preferred embodiment of the present invention, the antioxidant in the step 1 is mixed by two kinds of phenolic antioxidants.
Utilized viscosity grade according to the mineral oil in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 1 is 35～55.
Utilized viscosity grade according to the mineral oil in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 1 is 50.
According to the substrate thickness in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 1 is 1～5mm.
According to the substrate thickness in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 1 is 3mm.
Form the temperature difference of every group of chill roll by some groups of chill rolls according to the cooling forming machine in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 3.
According to the extractant in the extraction tank in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 5 is the alkanes extractant of 98%～99.5% high concentration.
According to the extractant in the extraction tank in the described lithium ion battery separator preparation method of the preferred embodiment of the present invention step 5 is a kind of in positive flow silane, normal heptane, the carrene.
The present invention also proposes a kind of lithium ion battery separator preparation system, comprise the agitating device that fully stirs with the speed of 40～300rpm in order to a certain proportion of ultra high molecular polyethylene, crosslinking agent, antioxidant and mineral oil, wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35; In order to extruding continuously with 100～250 ℃ of heating through the agitating device mixture after being mixed, form the extrusion device of substrate, it links to each other with agitating device; With so that the substrate that extrusion device is extruded passes through with 2～20 meters/minute speed, and substrate is carried out the cooling forming device of cooling forming with 5～40 ℃ temperature range, it links to each other with extrusion device; In order to speed the substrate through the cooling forming device cooling forming is carried out horizontal stroke, vertical two-way simultaneous stretching with 2～20 meters/minute, making substrate be drawn into thickness is that 30～100 μ m, acupuncture intensity are the biaxial tension device of the film of 300～600gf, and it links to each other with cooling forming device; Carry out single extraction in order to the film to biaxial tension device drawing and forming, and extract the extraction equipment of film mineral oil in fluid, it links to each other with the biaxial tension device; In order to the stripped film of extraction equipment under 100～160 ℃ temperature to carrying out 1～3 minute heat treated annealing device, it links to each other with extraction equipment; Curl in order to the film that annealing device was handled, and cut the packing device of cutting of packing, it links to each other with annealing device.
With respect to prior art, the present invention has the following advantages:
1, the present invention is adding antioxidant aspect the raw material use, and antioxidant can prolong film useful life, and battery diaphragm is to use at inside battery, prolongs barrier film and has guaranteed that not only battery is safe in utilization useful life, has also guaranteed the useful life of battery.
2, the present invention has used the cooling forming machine in the lithium ion battery separator preparation flow, and it can be with film moulding before stretching.Use the purpose of cooling forming machine also to be to make the ultra high molecular polyethylene in the raw material non-crystallizable behind high temperature, Film Thickness Ratio is more even like this, and the thickness homogeneity of the film of pulling out in the time of biaxial tension is relatively good, can stretched 12 microns slimline battery.
3, lithium ion battery separator preparation flow of the present invention has only used single extraction technology, has reduced the use of extractant, has reduced cost.
4, utilize the thickness deviation of the battery diaphragm of explained hereafter of the present invention can be controlled in the micron, the homogeneity of thickness is better.
5, utilize the battery diaphragm of explained hereafter of the present invention, the closed temperature of barrier film can reach the 130-170 degree.
6, utilize the battery diaphragm fusion temperature of explained hereafter of the present invention can reach the 130-160 degree.
7, utilize the battery diaphragm through-hole rate of explained hereafter of the present invention to be 30-70%.
Description of drawings
Fig. 1 is a kind of lithium ion battery separator preparation system structure chart of the embodiment of the invention;
Fig. 2 is the chemical structural formula of anti-oxidant Irganox.
Embodiment
Embodiment 1, and a kind of lithium ion battery separator preparation method's step is as follows in the present embodiment:
One, the speed with 40～300rpm in ultra high molecular polyethylene, crosslinking agent, antioxidant and the mineral oil proportioning adding by a certain percentage mixer is fully stirred raw material, wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35.
Antioxidant in the present embodiment can adopt phenolic antioxidant Irganox and 2,6 di tert butyl 4 methyl phenol, the chemical structural formula of anti-oxidant Irganox as shown in Figure 2, its molecular weight is 1178.Crosslinking agent is a polynorbornene.The molecular weight of the molecule of ultra high molecular polyethylene is 7,000,000～1,000,000.
Two, will drop into double screw extruder by the step 1 mixture after being mixed and extrude continuously, form substrate with 100～250 ℃ of heating.
Here the screw diameter of double screw extruder is 10～120 millimeters, its extrusion capacity greater than 260 kilograms per hour, mode of heating is segmented heating.
Three, making the substrate extruded from double screw extruder with 2～20 meters/minute speed is that 5～40 ℃ cooling forming machine carries out cooling forming by temperature range.
Four, with 2～20 meters/minute speed substrate is carried out horizontal stroke, vertical two-way simultaneous stretching by biaxial tension equipment, make substrate be drawn into film, the film thickness of drawing and forming reaches 30～100 μ m, and barrier film acupuncture intensity is 300～600gf.
Five, being 1500～2500 film with width extracts mineral oil in the film and one-step pore-creating by extraction tank.
Six, under 100～160 ℃ temperature, film carried out 1～3 minute heat treatment.
Seven, curling lithium battery diaphragm is cut packing.
The lithium ion battery separator fenestra that makes according to said method is evenly distributed, the fenestra through-hole rate between 30%～70%, fenestra size homogeneous, average pore size is between 0.03～0.065 micron, lithium ion battery separator at high temperature shrinkage ratio is less.In the present embodiment, antioxidant is that a class can suppress or slow down the material of macromolecular material autoxidation reaction speed, and it can guarantee that as stabilizer thermal oxidative degradation does not at high temperature take place battery diaphragm, can guarantee that hot conditions lower diaphragm plate shrinkage ratio is less.In addition, present embodiment can be regulated hot strength by regulating stretch ratio, thereby can guarantee that film thickness is even when carrying out the transverse and longitudinal stretching, and the transverse and longitudinal stretch ratio can be adjusted according to the thickness degree.
Embodiment 2, and the molecular weight of the ultra high molecular polyethylene of present embodiment in step 1 is 5,000,000, and other are identical with embodiment 1.
Embodiment 3, and the molecular weight of the ultra high molecular polyethylene of present embodiment in step 1 is 3,000,000, and other are identical with embodiment 1.
Embodiment 4, and the antioxidant of present embodiment in step 1 is mixed by two kinds of phenolic antioxidants, and other are identical with embodiment 1.
Embodiment 5, and the crosslinking agent of present embodiment in step 1 is polynorbornene, and the mass ratio of crosslinking agent and mineral oil is 1: 30-35, other are identical with embodiment 1.
Embodiment 6, and the utilized viscosity grade of the mineral oil of present embodiment in step 1 is 35～55, and other are identical with embodiment 1.
Embodiment 7, and the utilized viscosity grade of the mineral oil of present embodiment in step 1 is 50, and other are identical with embodiment 1.
Embodiment 8, and the utilized viscosity grade of the mineral oil of present embodiment in step 1 is 36, and other are identical with embodiment 1.
Embodiment 9, and the substrate thickness of present embodiment in step 1 is 1～5mm, and other are identical with embodiment 1.
Embodiment 10, and the substrate thickness of present embodiment in step 1 is 3mm, and other are identical with embodiment 1.
Embodiment 11, and the cooling forming machine of present embodiment in step 3 is made up of six groups of chill rolls, the temperature difference of every group of chill roll, and other are identical with embodiment 1.
Embodiment 12, and the extractant in the extraction tank of present embodiment in step 5 is the alkanes extractant of 98%～99.5% high concentration, and other are identical with embodiment 1.
Embodiment 13, and the extractant in the extraction tank of present embodiment in step 5 is a kind of in 98%～99.5% high concentration positive flow silane, normal heptane, the carrene, and other are identical with embodiment 1.
Table 1 and table 2 are respectively the index of the lithium ion battery separator of 16 μ m and 12 μ m.
Table 1
Table 2
The present invention also proposes a kind of lithium ion battery separator preparation system, and as shown in Figure 1, it is a kind of lithium ion battery separator preparation system structure chart of the embodiment of the invention.This lithium ion battery separator preparation system comprises agitating device 103, extrusion device 105, cooling forming device 107, biaxial tension device 109, extraction equipment 111, annealing device 113, cuts packing device 115.And agitating device 103, extrusion device 105, cooling forming device 107, biaxial tension device 109, extraction equipment 111, annealing device 113, cut packing device 115 and connect successively.
When lithium ion battery separator preparation system of the present invention is worked, at first the speed with 40～300rpm in a certain proportion of ultra high molecular polyethylene, crosslinking agent, antioxidant and the mineral oil adding agitating device 103 is fully stirred.Wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, and the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35.The molecular weight of ultra high molecular polyethylene is between 1,000,000 to 7,000,000.Crosslinking agent is a polynorbornene.Antioxidant is mixed by two kinds of phenolic antioxidant Irganox and 2,6 di tert butyl 4 methyl phenol, and it can guarantee that as stabilizer thermal oxidative degradation does not at high temperature take place battery diaphragm, can guarantee that hot conditions lower diaphragm plate shrinkage ratio is less.The utilized viscosity grade of mineral oil is between 35～55.Wherein, the chemical structural formula of anti-oxidant Irganox as shown in Figure 2, its molecular weight is 1178.
Through after the abundant stirring of agitating device 103, its mixture is added extrusion device 105 at ultra high molecular polyethylene, crosslinking agent, antioxidant and mineral oil, and extrude continuously with 100～250 ℃ of heating, form substrate, the thickness of this substrate is 1～5mm.Wherein extrusion device 105 can be a double screw extruder, and its screw diameter is 10～120 millimeters, extrusion capacity greater than 260 kilograms per hour, mode of heating is segmented heating, the temperature of head generally can be 100～160 ℃.
After extrusion device 105 is extruded substrate, the substrate of extruding is passed through cooling forming device 107 with 2～20 meters/minute speed, and substrate is carried out cooling forming with 5～40 ℃ temperature range.Cooling forming device 107 can be made up of six groups of chill rolls, the temperature difference of every group of chill roll, and cooling forming can make in the substrate ultra high molecular polyethylene non-crystallizable, reaches the purpose of film thickness homogeneous.
Behind substrate process cooling forming device 107 cooling formings, carry out horizontal stroke, vertical two-way simultaneous stretching by biaxial tension device 109 with 2～20 meters/minute speed again, making substrate be drawn into thickness is that 30～100 μ m, acupuncture intensity are the film of 300～600gf.Biaxial tension device 109 stretches simultaneously for transverse and longitudinal, can regulate hot strength by regulating stretch ratio, can guarantee that like this film thickness is even, and the transverse and longitudinal stretch ratio can be adjusted according to the thickness degree.
Behind film process biaxial tension device 109 drawing and formings, carry out single extraction through extraction equipment 111 again, and extract the mineral oil in the film.Extraction equipment 111 can be an extraction tank.Extractant in the extraction equipment 111 can be positive flow silane, normal heptane, carrene etc., and wherein the extractant of alkanes can make the mineral oil 99% in the film separate out fully.
Film through extraction equipment 111 extraction after, again by annealing device 113 with its under 100～160 ℃ temperature to carrying out heat treatment in 1～3 minute.
By cutting packing device 115 film is cut packing at last.
With respect to prior art, the present invention has the following advantages:
1, the present invention is adding antioxidant aspect the raw material use, and antioxidant can prolong film useful life, and battery diaphragm is to use at inside battery, prolongs barrier film and has guaranteed that not only battery is safe in utilization useful life, has also guaranteed the useful life of battery.
2, the present invention has used the cooling forming machine in the lithium ion battery separator preparation flow, and it can be with film moulding before stretching.Use the purpose of cooling forming machine also to be to make the ultra high molecular polyethylene in the raw material non-crystallizable behind high temperature, Film Thickness Ratio is more even like this, and the thickness homogeneity of the film of pulling out in the time of biaxial tension is relatively good, can stretched 12 microns slimline battery.
3, lithium ion battery separator preparation flow of the present invention has only used single extraction technology, has reduced the use of extractant, has reduced cost.
4, utilize the thickness deviation of the battery diaphragm of explained hereafter of the present invention can be controlled in the micron, the homogeneity of thickness is better.
5, utilize the battery diaphragm of explained hereafter of the present invention, the closed temperature of barrier film can reach the 130-170 degree.
6, utilize the battery diaphragm fusion temperature of explained hereafter of the present invention can reach the 130-160 degree.
7, utilize the battery diaphragm through-hole rate of explained hereafter of the present invention to be 30-70%.
More than disclosed only be several specific embodiment of the present invention, but the present invention is not limited thereto, any those skilled in the art can think variation, all should drop in protection scope of the present invention.
Claims (10)
1, a kind of lithium ion battery separator preparation method is characterized in that, may further comprise the steps:
One, the speed with 40～300rpm in ultra high molecular polyethylene, crosslinking agent, antioxidant and the mineral oil proportioning adding by a certain percentage mixer is fully stirred raw material, wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35;
Two, will drop into double screw extruder by the step 1 mixture after being mixed and extrude continuously, form substrate with 100～250 ℃ of heating;
Three, making the substrate extruded from double screw extruder with 2～20 meters/minute speed is that 5～40 ℃ cooling forming machine carries out cooling forming by temperature range;
Four, with 2～20 meters/minute speed substrate is carried out horizontal stroke, vertical two-way simultaneous stretching by biaxial tension equipment, make substrate be drawn into film, the film thickness of drawing and forming reaches 30～100 μ m, and barrier film acupuncture intensity is 300～600gf;
Five, be that 1500～2500 millimeters film extracts mineral oil in the film by extraction tank with width;
Six, under 100～160 ℃ temperature, film carried out 1～3 minute heat treatment;
Seven, curling lithium battery diaphragm is cut packing.
2, lithium ion battery separator preparation method as claimed in claim 1 is characterized in that, the antioxidant in the described step 1 is mixed by two kinds of phenolic antioxidants.
3, lithium ion battery separator preparation method as claimed in claim 1 is characterized in that, the utilized viscosity grade of the mineral oil in the described step 1 is 35～55.
4, lithium ion battery separator preparation method as claimed in claim 3 is characterized in that, the utilized viscosity grade of the mineral oil in the described step 1 is 50.
5, lithium ion battery separator preparation method as claimed in claim 1 is characterized in that, the substrate thickness in the described step 2 is 1～5mm.
6, lithium ion battery separator preparation method as claimed in claim 5 is characterized in that, the substrate thickness in the described step 2 is 3mm.
7, lithium ion battery separator preparation method as claimed in claim 1 is characterized in that, the cooling forming machine in the described step 3 is made up of some groups of chill rolls, the temperature difference of every group of chill roll.
8, lithium ion battery separator preparation method as claimed in claim 1 is characterized in that, the extractant in the described step 5 in the extraction tank is the alkanes extractant of 98%～99.5% high concentration.
9, lithium ion battery separator preparation method as claimed in claim 8 is characterized in that, the extractant in the described step 5 in the extraction tank is a kind of in positive flow silane, normal heptane, the carrene.
10, a kind of lithium ion battery separator preparation system is characterized in that, comprising:
In order to the agitating device that a certain proportion of ultra high molecular polyethylene, antioxidant and mineral oil are fully stirred with the speed of 40～300rpm, wherein, the mass ratio of mineral oil and antioxidant is 1500～1600: 1, the mass ratio of mineral oil and ultra high molecular polyethylene is 4～8: 1, and the mass ratio of crosslinking agent and mineral oil is 1: 30～35;
In order to extruding continuously with 100～250 ℃ of heating through this agitating device mixture after being mixed, form an extrusion device of substrate, it links to each other with this agitating device;
With so that the substrate that this extrusion device is extruded passes through with 2～20 meters/minute speed, and substrate is carried out a cooling forming device of cooling forming with 5～40 ℃ temperature range, it links to each other with this extrusion device;
In order to speed the substrate through this cooling forming device cooling forming is carried out horizontal stroke, vertical two-way simultaneous stretching with 2～20 meters/minute, making substrate be drawn into thickness is that 30～100 μ m, acupuncture intensity are a two-way stretching device of the film of 300～600gf, and it links to each other with this cooling forming device;
Carry out single extraction in order to the film to this biaxial tension device drawing and forming, and extract an extraction equipment of film mineral oil in fluid, it links to each other with this biaxial tension device;
In order to the stripped film of this extraction equipment under 100～160 ℃ temperature to carrying out 1～3 minute heat treated annealing device, it links to each other with this extraction equipment;
Curl in order to the film that this annealing device was handled, and cut one of packing and cut packing device, it links to each other with this annealing device.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102136557A (en) * | 2011-02-22 | 2011-07-27 | 上海双奥能源技术有限公司 | Lithium ion battery diaphragm and preparation method thereof |
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| CN102315404A (en) * | 2011-08-30 | 2012-01-11 | 上海乾呈玩具科技有限公司 | Preparation method and system for power lithium ion battery diaphragm |
| CN102569695A (en) * | 2010-12-14 | 2012-07-11 | 屠兆辉 | Preparation method for battery diaphragm |
| CN102555218A (en) * | 2010-12-14 | 2012-07-11 | 屠兆辉 | Method and system for preparing power lithium ion battery diaphragm |
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| WO2013078890A1 (en) * | 2011-12-02 | 2013-06-06 | 佛山市金辉高科光电材料有限公司 | Method for preparing power lithium battery diaphragm |
| CN106170509A (en) * | 2013-12-06 | 2016-11-30 | 东丽电池隔膜株式会社 | Polyolefin micro porous polyolefin membrane, nonaqueous electrolytic solution system secondary cell barrier film, polyolefin micro porous polyolefin membrane coiling body, nonaqueous electrolytic solution system secondary cell and the manufacture method of polyolefin micro porous polyolefin membrane |
| US9546253B2 (en) | 2010-08-05 | 2017-01-17 | Nitto Denko Corporation | Polyolefin porous film, method for producing the same and apparatus for producing the same |
| CN106450111A (en) * | 2016-11-24 | 2017-02-22 | 界首市天鸿新材料股份有限公司 | Dry-method dual-pulling process of high-performance lithium battery diaphragm |
| CN109326761A (en) * | 2018-08-10 | 2019-02-12 | 泰州衡川新能源材料科技有限公司 | For manufacturing the composition of lithium battery diaphragm |
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| CN109560235A (en) * | 2018-12-05 | 2019-04-02 | 河北金力新能源科技股份有限公司 | A kind of new type lithium ion battery aramid fiber diaphragm preparation method |
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2008
- 2008-08-25 CN CN2008100420430A patent/CN101345296B/en not_active Expired - Fee Related
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| US9546253B2 (en) | 2010-08-05 | 2017-01-17 | Nitto Denko Corporation | Polyolefin porous film, method for producing the same and apparatus for producing the same |
| CN102569695A (en) * | 2010-12-14 | 2012-07-11 | 屠兆辉 | Preparation method for battery diaphragm |
| CN102555218A (en) * | 2010-12-14 | 2012-07-11 | 屠兆辉 | Method and system for preparing power lithium ion battery diaphragm |
| CN102569695B (en) * | 2010-12-14 | 2014-07-30 | 屠兆辉 | Preparation method for battery diaphragm |
| CN102555218B (en) * | 2010-12-14 | 2014-09-24 | 屠兆辉 | Method and system for preparing power lithium ion battery diaphragm |
| CN102136557A (en) * | 2011-02-22 | 2011-07-27 | 上海双奥能源技术有限公司 | Lithium ion battery diaphragm and preparation method thereof |
| CN102136557B (en) * | 2011-02-22 | 2013-09-04 | 上海双奥能源技术有限公司 | Lithium ion battery diaphragm and preparation method thereof |
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| CN102208586B (en) * | 2011-04-18 | 2013-09-18 | 上海乾呈玩具科技有限公司 | Method and system for preparing dynamic lithium ion battery diaphragm |
| CN102315404A (en) * | 2011-08-30 | 2012-01-11 | 上海乾呈玩具科技有限公司 | Preparation method and system for power lithium ion battery diaphragm |
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| WO2013078890A1 (en) * | 2011-12-02 | 2013-06-06 | 佛山市金辉高科光电材料有限公司 | Method for preparing power lithium battery diaphragm |
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| CN106450111B (en) * | 2016-11-24 | 2019-07-26 | 界首市天鸿新材料股份有限公司 | The double drawing process of high-performance lithium battery diaphragm dry method |
| CN106450111A (en) * | 2016-11-24 | 2017-02-22 | 界首市天鸿新材料股份有限公司 | Dry-method dual-pulling process of high-performance lithium battery diaphragm |
| CN113471626A (en) * | 2018-07-18 | 2021-10-01 | 河南义腾新能源科技有限公司 | Polyethylene diaphragm and preparation method thereof |
| CN109326761A (en) * | 2018-08-10 | 2019-02-12 | 泰州衡川新能源材料科技有限公司 | For manufacturing the composition of lithium battery diaphragm |
| CN109326760A (en) * | 2018-08-10 | 2019-02-12 | 泰州衡川新能源材料科技有限公司 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
| CN109560235A (en) * | 2018-12-05 | 2019-04-02 | 河北金力新能源科技股份有限公司 | A kind of new type lithium ion battery aramid fiber diaphragm preparation method |
| CN109560235B (en) * | 2018-12-05 | 2022-04-22 | 河北金力新能源科技股份有限公司 | Novel preparation method of aramid fiber diaphragm of lithium ion battery |
| CN110838566A (en) * | 2019-11-06 | 2020-02-25 | 江苏厚生新能源科技有限公司 | Preparation method of multilayer polyethylene diaphragm |
| CN111081949A (en) * | 2019-12-31 | 2020-04-28 | 溧阳月泉电能源有限公司 | Cross-linked polyolefin diaphragm and preparation method thereof |
| CN111497293A (en) * | 2020-03-31 | 2020-08-07 | 江苏厚生新能源科技有限公司 | Preparation method of high-wettability film, high-wettability film and application thereof |
| CN111497293B (en) * | 2020-03-31 | 2022-04-05 | 江苏厚生新能源科技有限公司 | Preparation method of high-wettability film, high-wettability film and application thereof |
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